EP2814610B1 - Dispositifs en polymère ayant une microstructure - Google Patents
Dispositifs en polymère ayant une microstructure Download PDFInfo
- Publication number
- EP2814610B1 EP2814610B1 EP13706942.3A EP13706942A EP2814610B1 EP 2814610 B1 EP2814610 B1 EP 2814610B1 EP 13706942 A EP13706942 A EP 13706942A EP 2814610 B1 EP2814610 B1 EP 2814610B1
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- EP
- European Patent Office
- Prior art keywords
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- substrate
- microfluidic channel
- liquid
- Prior art date
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- 229920000642 polymer Polymers 0.000 title description 35
- 239000007788 liquid Substances 0.000 claims description 132
- 239000000758 substrate Substances 0.000 claims description 68
- 239000002904 solvent Substances 0.000 claims description 63
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- 238000000034 method Methods 0.000 claims description 42
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 10
- 229920000620 organic polymer Polymers 0.000 claims description 10
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- 238000004519 manufacturing process Methods 0.000 claims description 9
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- 238000001704 evaporation Methods 0.000 claims description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
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- 125000003700 epoxy group Chemical group 0.000 description 8
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 8
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
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- 150000001298 alcohols Chemical class 0.000 description 6
- 239000004020 conductor Substances 0.000 description 6
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- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 6
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- SOUHUMACVWVDME-UHFFFAOYSA-N safranin O Chemical compound [Cl-].C12=CC(N)=CC=C2N=C2C=CC(N)=CC2=[N+]1C1=CC=CC=C1 SOUHUMACVWVDME-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 5
- 125000002837 carbocyclic group Chemical group 0.000 description 5
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 5
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 5
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- 239000010457 zeolite Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 4
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- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 4
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N p-toluenesulfonic acid Substances CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 4
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- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
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- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 3
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
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- 238000013461 design Methods 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- 125000003277 amino group Chemical group 0.000 description 2
- 150000004982 aromatic amines Chemical class 0.000 description 2
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- GPRLTFBKWDERLU-UHFFFAOYSA-N bicyclo[2.2.2]octane Chemical compound C1CC2CCC1CC2 GPRLTFBKWDERLU-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
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- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
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- 230000037361 pathway Effects 0.000 description 1
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
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- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 235000013580 sausages Nutrition 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
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- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
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- BUUPQKDIAURBJP-UHFFFAOYSA-N sulfinic acid Chemical compound OS=O BUUPQKDIAURBJP-UHFFFAOYSA-N 0.000 description 1
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- GKLVYJBZJHMRIY-UHFFFAOYSA-N technetium atom Chemical compound [Tc] GKLVYJBZJHMRIY-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- XBFJAVXCNXDMBH-UHFFFAOYSA-N tetracyclo[6.2.1.1(3,6).0(2,7)]dodec-4-ene Chemical compound C1C(C23)C=CC1C3C1CC2CC1 XBFJAVXCNXDMBH-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 125000005000 thioaryl group Chemical group 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- 150000003672 ureas Chemical class 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/447—Systems using electrophoresis
- G01N27/44756—Apparatus specially adapted therefor
- G01N27/44791—Microapparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/107—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by filling grooves in the support with conductive material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1258—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns by using a substrate provided with a shape pattern, e.g. grooves, banks, resist pattern
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2300/00—Additional constructional details
- B01L2300/06—Auxiliary integrated devices, integrated components
- B01L2300/0627—Sensor or part of a sensor is integrated
- B01L2300/0645—Electrodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2300/00—Additional constructional details
- B01L2300/08—Geometry, shape and general structure
- B01L2300/0809—Geometry, shape and general structure rectangular shaped
- B01L2300/0816—Cards, e.g. flat sample carriers usually with flow in two horizontal directions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/04—Moving fluids with specific forces or mechanical means
- B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
- B01L2400/0415—Moving fluids with specific forces or mechanical means specific forces electrical forces, e.g. electrokinetic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/04—Moving fluids with specific forces or mechanical means
- B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
- B01L2400/0415—Moving fluids with specific forces or mechanical means specific forces electrical forces, e.g. electrokinetic
- B01L2400/0427—Electrowetting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502769—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements
- B01L3/502784—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements specially adapted for droplet or plug flow, e.g. digital microfluidics
- B01L3/502792—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements specially adapted for droplet or plug flow, e.g. digital microfluidics for moving individual droplets on a plate, e.g. by locally altering surface tension
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06K—GRAPHICAL DATA READING; PRESENTATION OF DATA; RECORD CARRIERS; HANDLING RECORD CARRIERS
- G06K19/00—Record carriers for use with machines and with at least a part designed to carry digital markings
- G06K19/06—Record carriers for use with machines and with at least a part designed to carry digital markings characterised by the kind of the digital marking, e.g. shape, nature, code
- G06K19/067—Record carriers with conductive marks, printed circuits or semiconductor circuit elements, e.g. credit or identity cards also with resonating or responding marks without active components
- G06K19/07—Record carriers with conductive marks, printed circuits or semiconductor circuit elements, e.g. credit or identity cards also with resonating or responding marks without active components with integrated circuit chips
- G06K19/077—Constructional details, e.g. mounting of circuits in the carrier
- G06K19/07749—Constructional details, e.g. mounting of circuits in the carrier the record carrier being capable of non-contact communication, e.g. constructional details of the antenna of a non-contact smart card
- G06K19/0775—Constructional details, e.g. mounting of circuits in the carrier the record carrier being capable of non-contact communication, e.g. constructional details of the antenna of a non-contact smart card arrangements for connecting the integrated circuit to the antenna
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1208—Pretreatment of the circuit board, e.g. modifying wetting properties; Patterning by using affinity patterns
Definitions
- This technology relates to methods for manufacturing devices having an electrode pattern formed thereon. It also relates to such devices.
- Microfluidic devices such as micro-structured polymer devices (MPDs) are useful tools for the analysis of chemicals and biological fluids.
- Microfluidic devices can be formed from plastics compounds, which may be formed by a moulding process.
- Microfluidic devices typically include fluid transport channels-for example input and output channels-and other fluid flow or storage structures to enable the intended measurement or chemical or biological reaction to take place. For effective analysis of the fluid by the microfluidic device the fluid must controllably pass through these channels.
- Microfluidic devices will often include electrodes, i.e. electrically conductive structures, arranged to interact with fluid in the channels or other fluid structures. Examples might be electrodes leading to a measurement sensor, to enable a property of a channel to be measured, and electrodes for receiving an active electrical stimulus, e.g. to receive a voltage signal for manipulating fluid in the MPD by electrowetting or dielectrophoresis.
- electrodes i.e. electrically conductive structures
- Examples might be electrodes leading to a measurement sensor, to enable a property of a channel to be measured, and electrodes for receiving an active electrical stimulus, e.g. to receive a voltage signal for manipulating fluid in the MPD by electrowetting or dielectrophoresis.
- Various types of microfluidic devices have been proposed.
- the channel cross-section dimensions in a microfluidic device can vary widely, but may be anything from the millimetre scale to the nanometre scale. Reference to microfluidics in this document is not restricted to micrometre scale devices,
- a basic form of a microfluidic device is based on continuous flow of the relevant fluids through the channels.
- a development of this basic form has the active fluid conveyed through the channels in droplets held in suspension by a functionally inert carrier liquid.
- Some of the devices described herein are droplet-based, microfluidic devices.
- a droplet is formed of a first liquid, the droplet liquid, suspended immiscibly in a second liquid, the carrier liquid.
- the droplet liquid and the carrier liquid should be selected to be immiscible over the relevant time scale needed for good functioning of the device as determined by factors such as transit time, storage time, and reaction time within the device.
- Droplets are generally spherical, but in use the droplets may be distorted by forces or constrained by boundaries of the channel or other parts of the microstructured device, so other shapes may exist.
- a droplet in the context of a digital microfluidic device is therefore a contiguous volume of a fluid held in a carrier liquid, wherein the fluid and the carrier liquid are immiscible.
- Microfluidic devices may be made from a variety of substrate materials, including thermoplastic, glass and crystal.
- the channels can be formed by a variety of means, including injection moulding.
- Known ink compositions contain non-volatile solvents, particularly high boiling point polyols such as glycerol.
- the boiling point of these solvents may range from 80 to 300° C., in some embodiments 100 to 200° C.
- These components act as humectants to prevent premature drying of the ink in the jetting nozzles to ensure reliability of the jetting process.
- the sintering is normally a heating step which evaporates the solvent of the conductive liquid.
- the presence of the high boiling point liquids influences the temperature of the sintering however as any remaining organic component will impede a conductive pathway, thereby producing a product with lower and more variable conductivity. Higher sintering temperatures require a greater energy input and may damage thermoplastic substrates.
- the invention is defined by claim 1.
- the primer layer absorbs the non-volatile components of the humectant organic solvents in which the electrically conductive material of the conductive liquid is dispersed, so that these components are no longer present in the ink but are absorbed into the primer layer.
- the composition of the primer layer acts as a sieve for the undesired ingredients in the conductive liquid, absorbing these components into the primer layer. This allows the final sintering step to be carried out at a lower temperature than was previously possible in the art. This is particularly applicable when the substrate is formed of a thermoplastic polymer, especially a polyolefin such as cycloolefin polymer.
- the primer layer can be applied using a primer liquid and capillary action, similar to how the conductive liquid is applied.
- the primer liquid can be introduced to the microfluidic channel structure, for example a droplet can be placed at one or more specific locations in or adjacent to the channel structure, and then allowed to flow by capillary action over the primer layer throughout the micro fluidic channel structure.
- the primer layer can be applied by deposition into the microfluidic channel, e.g. by a printing process such as screen printing or inkjet printing, or evaporation through a mask.
- alkyl denotes a straight- or branched-chain, saturated, aliphatic hydrocarbon radical. Said “alkyl” may consist of 1 to 12, typically 1 to 8, in some embodiments 1 to 6 carbon atoms.
- a C1-6 alkyl group includes methyl, ethyl, propyl, isopropyl, butyl, t-butyl, 2-butyl, pentyl, hexyl, and the like. The alkyl group may be substituted where indicated herein.
- Cycloalkyl denotes a cyclic, saturated, aliphatic hydrocarbon radical.
- Examples of cycloalkyl groups are moieties having 3 to 10, for example 3 to 8 carbon atoms including cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and cyclooctyl groups.
- the cycloalkyl group may be substituted where indicated herein.
- Alkoxy means the radical “alkyl-O-", wherein “alkyl” is as defined above, either in its broadest aspect or a more restricted aspect.
- Phenyl means the radical -C6H5. The phenyl group may be substituted where indicated herein.
- Haldroxy means the radical -OH.
- Thiol means the radical -SH.
- Halo means a radical selected from fluoro, chloro, bromo, or iodo.
- Niro means the radical -NO2.
- Carboxylic acid means the radical -CO2H.
- Sulfonic acid means the radical -SO3H.
- Amino means the radical -NR2, wherein R is hydrogen or alkyl (as defined above, either in its broadest aspect or a more restricted aspect).
- the device of the present technology has a planar electrode structure and is formed on a substrate.
- the substrate is not particularly critical to the present technology provided it is compatible with the primer layer and the conductive liquid.
- suitable substrates include glasses, particularly epoxy glasses, and thermoplastic organic polymers.
- the substrate is a thermoplastic organic polymer.
- Suitable thermoplastic organic polymers that can be used to provide the substrate include, but are not limited to, polymers formed from monomers having ethylenically unsaturated groups (in particular polyolefins), polyamides (nylons), polyesters, polycarbonates, polyimides and mixtures thereof.
- suitable polymers formed from ethylenically unsaturated monomers include polyolefins, which include, but are not limited to: polyethylenes; polypropylenes; poly(1-butene); poly(methyl pentene); poly(vinyl chloride); poly(acrylonitrile); poly(tetrafluoroethylene) (PTFE-Teflon®), poly(vinyl acetate); polystyrene; poly(methyl methacrylate); ethylene-vinyl acetate copolymer; ethylene methyl acrylate copolymer; styreneacrylonitrile copolymers; cycloolefin polymers and copolymers; and mixtures and derivatives thereof.
- suitable polyethylenes include, but are not limited to, low density polyethylene, linear low density polyethylene, high density polyethylene, ultra-high molecular weight polyethylene, and derivatives thereof.
- suitable polyamides include nylon 6-6, nylon 6-12 and nylon 6.
- suitable polyesters include polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, polyethylene adipate, polycaprolactone, and polylactic acid.
- the thermoplastic organic polymer is a polyolefin, in particular. a cycloolefin homopolymer or copolymer.
- cycloolefin homopolymer means a polymer formed entirely from cycloalkene (cycloolefin) monomers.
- the cycloalkene monomers from which the cycloolefin homopolymer is formed have 3 to 14, in some embodiments 4 to 12, in some embodiments 5 to 8, ring carbon atoms.
- the cycloalkene monomers from which the cycloolefin homopolymer is formed have 1 to 5, such as 1 to 3, in some embodiments 1 or 2, in some embodiments 1 carbon-carbon double bonds.
- the cycloalkene monomers from which the cycloolefin homopolymer is formed have 1 to 5, such as 1 to 3, in some embodiments 1 or 2, in some embodiments 1 carbocyclic ring.
- the carbocyclic ring may be substituted with one or more, typically 1 to 3, in some embodiments 1 or 2, in some embodiments 1 substituent, the substituent(s) being each independently selected from the group consisting of C1-6 alkyl (typically C1-4 alkyl, particularly methyl or ethyl), C3-8 cycloalkyl (typically C5-7 cycloalkyl, especially cyclopentyl or cyclohexyl), phenyl (optionally substituted by 1 to 5 substituents selected from C1-6 alkyl, C1-6 alkoxy, halo and nitro), or halogen.
- C1-6 alkyl typically C1-4 alkyl, particularly methyl or ethyl
- C3-8 cycloalkyl typically C5-7 cycloalkyl, especially
- cycloolefin copolymer means a polymer formed from both cycloalkene and non-cyclic alkene (olefin) monomers.
- the cycloalkene monomers from which the cycloolefin copolymer is formed have 3 to 14, in some embodiments 4 to 12, in some embodiments 5 to 8, ring carbon atoms.
- the cycloalkene monomers from which the cycloolefin coopolymer is formed have 1 to 5, such as 1 to 3, in some embodiments 1 or 2, in some embodiments 1 carbon-carbon double bonds.
- the cycloalkene monomers from which the cycloolefin copolymer is formed have 1 to 3, in some embodiments 1 or 2, in some embodiments 1 carbocyclic ring.
- the carbocyclic ring may be substituted with one or more, typically 1 to 3, in some embodiments 1 or 2, in some embodiments 1 substituent, the substituent(s) being each independently selected from the group consisting of C1-6 alkyl (typically C1-4 alkyl, particularly methyl or ethyl), C3-8 cycloalkyl, (typically C5-7 cycloalkyl, especially cyclopentyl or cyclohexyl), phenyl (optionally substituted by 1 to 5 substituents selected from C1-6 alkyl, C1-6 alkoxy, halo and nitro), or halogen.
- C1-6 alkyl typically C1-4 alkyl, particularly methyl or ethyl
- C3-8 cycloalkyl typically C5-7 cycloalkyl, especially cyclopent
- non-cyclic alkene copolymerised with the cycloolefin examples include ethylene; propylene; 1-butene; 2-methylpentene; vinyl chloride; acrylonitrile; tetrafluoroethylene; vinyl acetate; styrene; methyl methacrylate and methyl acrylate, in some embodiments ethylene or propylene, particularly ethylene.
- cycloolefin homopolymers and copolymers usable in the present technology are those based on 8,8,10-trinorborn-2-ene (norbornene; bicyclo[2.2.1]hept-2-ene) or 1,2,3,4,4a,5,8,8a-octahydro-1,4:5,8-dimethanonapthalene (tetracyclododecene) as monomers.
- homopolymers of these monomers can be formed by a ring opening metathesis polymerisation: copolymers are formed by chain copolymerisation of the aforementioned monomers with ethylene.
- the cycloolefin polymer is a cycloolefin homopolymer of general formula (A): wherein:
- Ra and Rb are each independently selected from the group consisting of hydrogen, C1-6 alkyl, C3-8 cycloalkyl or phenyl. In one embodiment, Ra and Rb are each independently selected from the group consisting of hydrogen or C1-6 alkyl. In one embodiment, Ra and Rb are both hydrogen.
- Ra and Rb together with the carbon atoms to which they are attached form a ring selected from cyclopentane, cyclohexane, cycloheptane, cyclooctane, bicyclo[2.2.1]heptane or bicyclo[2.2.2]octane, the ring carbon atoms each being optionally substituted by one or more substituents selected from the group consisting of C1-6 alkyl, C3-8 cycloalkyl or phenyl.
- m is such that the average molecular weight (Mw) of the polymer ranges from 50,000 to 150,000.
- the cycloolefin polymer is a cycloolefin polymer of formula (B): wherein:
- n and 1 are such that the average molecular weight (Mw) of the polymer ranges from 50,000 to 150,000.
- n is such that the mole fraction of cycloolefin repeating units ranges from 0.3 to 0.6; and 1 is such that the mole fraction of ethylene repeating units ranges from 0.7 to 0.4.
- PDMS silicone polymers polydimethylsiloxane
- n is such that the average molecular weight (Mw) of the polymer ranges from 100 to 100,000, in some embodiments 100 to 50,000.
- suitable glasses that can be used to provide the substrate include silica glasses, in particular phosphosilicate glass compounds and borosilicate glass compounds.
- the substrate may be a glass-reinforced epoxy laminate.
- This is a composite material composed of woven fibreglass cloth with an epoxy resin binder.
- Such composite materials are generally known in the art under the grade designation FR-4.
- the fibreglass also called glass-reinforced plastic, glass-fibre reinforced plastic, or GFRP
- the polymer may be epoxy (as defined and exemplified below), a thermosetting plastic (in some embodiments polyester, as defined and exemplified above, or vinylester, which is a resin produced by the esterification of an epoxy resin with an unsaturated monocarboxylic acid) or thermoplastic (as defined and exemplified above).
- the epoxy resin used in this technology may be formed by copolymerising a resin with an activator.
- the resin consists of monomers or prepolymers having more than one epoxide group, the epoxide groups generally being present at terminal ends of the molecule.
- the activator is then applied to cleave the epoxy groups of the prepolymer and cross-link the polymer.
- a typical prepolymer resin is a compound of the formula: where n denotes the number of polymerized subunits and is in the range from 0 to about 25.
- the resin is formed by reacting an epoxy monomer with a polyol.
- the "epoxy monomer” is a compound having an epoxy group and a leaving group displaceable by a hydroxyl group (which may be, for example a halogen atom, such as chlorine, bromine or iodine, or a sulfonyloxy group, such as methanesulfonyloxy, benzenesulfonyloxy or p-toluenesulfonyloxy).
- a particular example of an epoxy monomer is epichlorohydrin.
- a polyol is an organic compound having more than one hydroxy group. In some embodiments, the polyol is a polyphenol, i.e.
- a particular example of a polyol is 4,4'-(propane-2,2-diyl)diphenol (bisphenol-A).
- bisphenol-A 4,4'-(propane-2,2-diyl)diphenol
- epoxy resins include multifunctional epoxy resins, alicyclic epoxy resins, brominated epoxy resins, and epoxy-novolac resins.
- the epoxy resin is not particularly limited provided it contains more than one epoxy group in the prepolymer molecule.
- the activator may be any activator conventionally used to cure epoxy resin prepolymers.
- Examples of the activator which reacts with the epoxy groups of the uncured epoxy resin prepolymer to cure the resin include amines, imidazoles, amides, esters, alcohols, thiols, ethers, thioethers, phenols, phosphorus compounds, ureas, thioureas, acid anhydrides, Lewis acids, onium salts, active silica compounds-aluminium complex.
- Suitable classes of amines include aliphatic amines, alicyclic and heterocyclic amines, aromatic amines, modified amines and the like.
- aliphatic amines include ethylenediamine, trimethylenediamine, tetramethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenediamine, dimethylamino-propylamine, diethylaminopropylamine, trimethylhexamethylenediamine, pentanediamine, bis(2-dimethylaminoethyl)ether, pentamethyldiethylenetriamine, alkyl-t-monoamine, 1,4-diazabicyclo(2.2.2)octane (triethylenediamine), N,N,N',N'-tetramethylhexamethylenediamine, N,N,N',N'-tetramethylpropylenediamine, N,N,N',N'-tetramethylethylenediamine, N,N-dimethylcyclohexylamine, dimethylamino-ethoxye
- alicyclic and heterocyclic amines examples include piperidine, menthanediamine, isophoronediamine, methylmorpholine, ethylmorpholine, N,N',N"-tris(dimethylaminopropyl)hexahydro-s-triazine, N-aminoethylpiperidine, trimethylaminoethyl-piperidine, bis(4-aminocyclohexyl)methane, N,N'-dimethylpiperidine and 1,8-diazabicyclo(4.5.0)undec-7-ene.
- aromatic amines examples include o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, benzylmethylamine, dimethylbenzylamine, m-xylenediamine, pyridine and picoline.
- modified polyamines include polyamines added with epoxy compounds, polyamines added by Michael reaction, polyamines added by Mannich reaction, polyamines added with thiourea and ketone-blocked polyamines.
- suitable amines include dicyandiamide, guanidine, organic acid hydrazides, diaminomaleonitrile, amineimide, trifluoroboron-piperidine complex and trifluoroboron-monoethylamine complex.
- imidazole compounds include imidazole, 2-methylimidazole, 2-ethylimidazole, 2-isopropylimidazole, 2-n-propylimidazole, 2-undecyl-1H-imidazole, 2-heptadecyl-1H-imidazole, 1,2-dimethylimidazole, 2-ethyl-4-methylimidazole, 2-phenyl-1H-imidazole, 4-methyl-2-phenyl-1H-imidazole, 2-phenyl-4-methylimidazole, 1-benzyl-2-methylimidazole, 1-cyanoethyl-2-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 1-cyanoethyl-2-undecylimidazole, 1-cyanoethyl-2-phenylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazolium trimellitate, 1-cyan
- imidazoline compounds examples include 2-methylimidazoline and 2-phenylimidazoline.
- amide compounds include polyamides obtainable by means of polymerization of a dicarboxylic acid and a polyamine.
- ester compounds include active carbonyl compounds, such as aryl and thioaryl esters of carboxylic acids.
- phenols, alcohols, thiols, ethers and thioether compounds include phenol novolac, cresol novolac, polyols, polymercaptans, polysulfides, 2-(dimethylaminomethylphenol), 2,4,6-tris(dimethylaminomethyl)phenol, and tri-2-ethylhexyl hydrochloride of 2,4,6-tris(dimethylaminomethyl)phenol.
- the activator is a polyamine monomer.
- the amine groups on the activator may be primary, secondary, tertiary, or a mixture thereof.
- suitable polyamines include ethylenediamine, diethylenetriamine, triethylene-tetramine, and diaminodiphenylmethane.
- Crystal substrates in particular semiconductor substrates, such as silicon substrates, may also be used.
- Another suitable crystal for the substrate is lithium niobate.
- the devices of the present technology also include a primer layer.
- the primer layer is then applied to at least part of the microfluidic channel.
- the primer layer is capable of absorbing the humectant organic solvent (particularly although not exclusively the higher boiling point components thereof) in which the metal particles of the conductive liquid are dispersed. This allows the subsequent sintering to be carried out at a much lower temperature than was previously possible in the art: this is particularly advantageous for thermoplastic substrates as it avoids overheating and possible damage to the substrate.
- the primer layer should also have a low viscosity (typically 5 to 500 mPa ⁇ s; in some embodiments 5 to 100 mPa ⁇ s) and should be soluble in and/or at least compatible with in the dispensing solvent used to obtain optimal fluidic flow into the channels.
- a low viscosity typically 5 to 500 mPa ⁇ s; in some embodiments 5 to 100 mPa ⁇ s
- the primer layer according to the present technology also includes a porous particulate material.
- the porous particulate material acts as a filler and further aids in the absorption of the humectant organic solvents (particularly the non-volatile components thereof) contained in the conductive liquid.
- the porous particulate material also serves to regulate the flow of the primer layer when dispensed into a microfluidic channel. Undesirable effects such as overflow of the primer into neighbouring regions on the fluidic device can be controlled by the appropriate choice and concentration of the porous particulate material.
- the porous particulate material comprises a molecular sieve.
- molecular sieve means a material containing pores of a precise and uniform size and which are capable of acting as an adsorbent for gases and liquids. Molecules small enough to pass through the pores are adsorbed while larger molecules, specifically metallic particles present in a conductive liquid jet ink, are not.
- the pore volume ranges from 0.20 to 1.20 ml/g, or in some embodiments from 0.40 to 0.60 ml/g.
- porous particulate materials include metal and semimetal oxides such as silica (especially amorphous silica), aluminas (including boehmite, aluminium oxide monohydrate and Bayerite, aluminium oxide trihydrate), titania, zeolites (porous aluminosilicate materials), barium sulphate and silica-alumina hydrates and oxides.
- metal and semimetal oxides such as silica (especially amorphous silica), aluminas (including boehmite, aluminium oxide monohydrate and Bayerite, aluminium oxide trihydrate), titania, zeolites (porous aluminosilicate materials), barium sulphate and silica-alumina hydrates and oxides.
- the porous particulate material is alumina boehmite, AlO(OH).
- alumina boehmites include the range of water dispersible alumina boehmites available as DISPERAL® and DISPAL® from Sasol.
- the alumina may be an organically modified alumina.
- the hydroxyl group on the boehmite may be etherified by substitution of the hydrogen with an alkyl group, or esterified by substitution of the hydrogen with an acyl group, which may be a carboxyl or sulfonyl group.
- alumina-modifying reagents for forming examples include alkylating agents, such as alkyl halides or sulfonates, acylating agents, such as carboxylic acid chlorides and carboxylic acid anhydrides, and sulfonylating agents, such as sulfonic acids, sulfonic acid chlorides and sulfonic acid anhydrides.
- alkylating agents such as alkyl halides or sulfonates
- acylating agents such as carboxylic acid chlorides and carboxylic acid anhydrides
- sulfonylating agents such as sulfonic acids, sulfonic acid chlorides and sulfonic acid anhydrides.
- a particular modifying reagent is p-toluenesulfonic acid.
- the porous particulate material is silica, especially fumed silica.
- the porous particulate material is a zeolite.
- Zeolites are porous aluminosilicate materials capable of acting as molecular sieves. Zeolites have a porous structure that can accommodate a wide variety of cations, such as Na+, K+, Ca2+, and Mg2+. These positive ions can readily be exchanged for others in a contact solution.
- zeolites examples include amicite, analcime, barrerite, bellbergite, bikitaite, boggsite, brewsterite, chabazite, clinoptilolite, cowlesite, dachiardite, edingtonite, epistilbite, erionite, faujasite, ferrierite, garronite, gismondine, gmelinite, gobbinsite, gonnardite, goosecreekite, harmotome, herschelite, heulandite, laumontite, levyne, maricopaite, mazzite, merlinoite, mesolite, montesommaite, mordenite, natrolite, offretite, paranatrolite, paulingite, pentasil (also known as ZSM-5), perlialite, phillipsite, pollucite, scolecite, sodium dachiardite, stellerite, stil
- the porous particulate material is typically present as a dispersion in a solvent.
- the solvent is water or a hydrophilic organic solvent such as an alcohol, an ether (particularly a glycol ether such as those described and exemplified below), a ketone or an ester.
- the solvent in which the porous particulate material is dispersed is water.
- the porous particulate material may be effective as a primer layer in the absence of an organic polymer. Therefore, in an alternative embodiment the primer layer consists essentially of a porous particulate material, as defined and exemplified above (either in its broadest aspect or a more restricted aspect) dispersed in a solvent as defined and exemplified above (either in its broadest aspect or a more restricted aspect).
- the primer layer comprises a porous particulate material without an organic polymer, the primer layer contains up to 50%, in some embodiments up to 40%, in some embodiments up to 30%, in some embodiments up to 25%, and in some embodiments up to 20% by weight of the porous particulate material (as a percentage by weight of the concentrated particulate material in the primer, the remainder comprising the solvent).
- the primer layer is generally applied to the substrate diluted in solution, in some embodiments in a hydrophilic/hydrophobic solvent.
- the solvent used to dilute the primer layer should in some embodiments exhibit a lower surface tension with respect to surface energy of the microfluidic substrate.
- the surfactant-like properties of the solvent, low surface tension and slow evaporation rate enables the formulated primer layer to flow across the region of the substrate only where it is intended to be applied.
- Suitable solvents include oxygenated solvents, such as alcohols, and ethers (particularly glycol ethers such as those defined and exemplified below), ketones and esters.
- the solvent in which the primer layer is diluted is a glycol ether.
- these solvents exhibit a good range of properties such as good solvency of hydrophilic and hydrophobic coating polymers, good flow behaviour on hydrophobic surfaces and controllable evaporation (drying).
- glycol ethers examples include: ethylene glycol mono(Cl-6)alkyl ethers such as ethylene glycol monopropyl ether, ethylene glycol monoisopropyl ether (isopropoxyethanol) and ethylene glycol monobutyl ether; ethylene glycol phenyl ether; diethylene glycol mono(C1-6)alkyl ethers such as diethylene glycol monomethyl ether, diethylene glycol monoethyl ether (CARBITOLTM), diethylene glycol monobutyl ether and diethylene glycol monohexyl ether; triethylene glycol mono(C1-6)alkyl ethers (alkoxytriglycols) such as triethylene glycol monomethyl ether (methoxytriglycol), triethylene glycol monoethyl ether (ethoxytriglycol) and triethylene glycol monobutyl ether (butoxytriglycol); propylene glycol (C1-6)alkyl ethers such as propylene glycol methyl
- ethylene glycol monoisopropyl ether isopropoxyethanol
- dipropylene glycol monomethyl ether and mixtures thereof.
- the primer layer is applied in a solution containing 50 to 95%, in some embodiments 60 to 90%, in some embodiments 65 to 80%, by weight of the concentrated primer layer and 5 to 50%, in some embodiments 10 to 40%, in some embodiments 20 to 35%, by weight of the diluting solvent.
- the devices of the present technology further comprise an electrically conductive pattern over the primer layer.
- step (c) comprises applying a conductive liquid over the primer layer and step (d) comprises allowing the conductive liquid to flow throughout the microfluidic channel by capillary action to form the planar electrode structure.
- the surface tension of the conductive liquid is lower than the surface energy of the receptive substrate.
- the properties of the conductive liquid should be such that it does not dry before complete coverage of the substrate is attained by fluid flow. Either or both (for example, both) of these properties assist in achieving complete fluidic flow, and therefore complete and homogeneous coverage of the channels with the conductive liquid.
- the conductive liquid comprises electrically conductive particles dispersed in a carrier medium.
- the electrically conductive material from which the particles are formed is a metal.
- the metal is not particularly limited provided it does not react with the solvents.
- suitable metals include alkaline earth metals such as beryllium, magnesium, calcium, strontium and barium; transition metals such as zinc, molybdenum, cadmium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, yttrium, zirconium, niobium, technetium, ruthenium, rhodium, palladium, silver, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum and gold; and p-block metals such as aluminium, gallium, indium, tin, thallium, lead and bismuth.
- Example metals include nickel, copper, palladium, tungsten,
- alloys or mixtures of two or more of the above-mentioned metals and other conductive compounds may be used.
- the conductive material is a conductive metal oxide.
- These materials are metal oxides doped with another metal in sufficient amounts to cause the material to be electrically conductive.
- Examples of conductive metal oxides include indium tin oxide (ITO), antimony tin oxide, indium-doped cadmium oxide and aluminium-doped zinc oxide.
- the conductive material is a conductive form of carbon.
- conductive forms of carbon include graphite and carbon nanotubes.
- the metallic or electrically conductive particles dispersed in the conductive liquid are nanoparticles.
- the particle size of the nanoparticles should be such that they are not absorbed into the primer layer.
- the particle size of the nanoparticles ranges from 5 to 200 nm, in some embodiments 50 to 150 nm.
- the conductive particles are dispersed in a carrier medium.
- the carrier medium includes a solvent.
- the solvent is not particularly critical provided that it permits the formation of a stable suspension of the conductive particles and can permits the conductive liquid to flow throughout the microfluidic channel by capillary action to form the planar electrode structure.
- the carrier medium additionally contains water.
- the solvent is an organic solvent, particularly a water-miscible organic solvent.
- the solvent has a surface tension and/or a boiling point which is particularly suited to facilitate fluidic flow of the suspension into the microfluidic channels.
- the solvent has a boiling point in the range of 80 to 300° C., in some embodiments 100 to 200° C.
- the solvent has a surface tension in the range of 10 to 45 mN/m, in some embodiments 20 to 40 mN/m.
- the conductive particles are dispersed in a carrier, which includes a solvent.
- Suitable classes of solvents include oxygenated solvents, such as alcohols (particularly polyols, i.e. alcohols containing more than one OH group), ethers, ketones and esters.
- oxygenated solvents such as alcohols (particularly polyols, i.e. alcohols containing more than one OH group), ethers, ketones and esters.
- Particular examples of solvents include:
- the solvent is ethylene glycol diacetate, which has a surface tension of 33 mN/m which is particularly suited to aiding capillary flow.
- the solvent is a mixture of water and dipropylene glycol monomethyl ether.
- the water and dipropylene glycol monomethyl ether are typically present in a mixing ratio of 10:90 to 90:10 by volume, in some embodiments 30:70 to 70:30 by volume.
- the solvent is a 50:50 (by volume) mixture of water and dipropylene glycol monomethyl ether, which has a surface tension of 33 mN/m which is particularly suited to aiding capillary flow.
- conductive liquids are commercially available from a number of sources.
- suitable conductive liquids are those available from Sun Chemical Corporation commercially available under the trade names EMD5603 and EMD5714.
- the conductive liquid may optionally further include a corrosion inhibitor.
- a corrosion inhibitor are required when the metal is non-noble (i.e. a metal other than ruthenium, rhodium, palladium, silver, osmium, iridium, platinum or gold) to prevent oxidation of the metal.
- corrosion inhibitors examples include hydrazine, amines such as hexamine, phenylenediamine or dimethylethanolamine or sterically hindered amines such as those described and exemplified below; quaternised amines, polyamines such as polyaniline; aldehydes such as cinnamaldehyde; imines; and inorganic corrosion inhibitors such as nitrites (eg sodium nitrite), chromates and phosphates; and mixtures of any thereof.
- amines such as hexamine, phenylenediamine or dimethylethanolamine or sterically hindered amines such as those described and exemplified below
- quaternised amines polyamines such as polyaniline
- aldehydes such as cinnamaldehyde
- imines and inorganic corrosion inhibitors
- nitrites eg sodium nitrite
- chromates and phosphates and mixtures of any
- the corrosion inhibitor is a sterically hindered amine.
- Suitable hindered amines include diethanolamine, triethanolamine, imidazole derivatives and their salts with polycarboxylic acids.
- Particularly suitable corrosion inhibitors are commercially available from BASF Corporation under the trade names Corrosion Inhibitor Amine O, Irgacor L184, and Irgacor L190 Plus. These are particularly suitable because of their solubility in hydrophilic formulations.
- FIGS. 1A to 1G are schematic sections through a substrate showing in sequence steps in the manufacture of an electrode in a channel (as an example feature of a microfluidic channel structure) according to an embodiment of the technology.
- the process is typically carried out under cleanroom conditions.
- the substrate is cleaned with a degreasing solvent (typically an isopropanol/water mixture).
- the substrate may be cleaned with compressed air to remove dust or contamination.
- FIG. 1A shows a substrate 10 having an upper or top surface 12 and a lower or bottom surface 14.
- the substrate 10 has a semi-circular section channel 20 formed in the upper surface 12, e.g. by moulding (such as injection moulding), stamping, machining or etching.
- the channel 20 is intended to define the location of an electrode, i.e. the purpose of the channel is for it to be used in fabrication of an electrode, as opposed to use as a flow channel in the final microfluidic device. Accordingly, the channel 20, as an example of a microfluidic channel structure, is shaped to match the desired electrode structure.
- FIG. 1B shows the channel 20 in a primer distribution phase during which the channel 20 is partly filled with a solution 22 which is a primer liquid comprising a primer solvent-containing primer carrier medium.
- the primer solution can be applied by micro-dispensing into the channel, e.g. with a syringe, micropipette or ink jet print head nozzle.
- the composition of the primer solution allows it to spread along the channel by capillary action, resulting in a smooth and even coverage of the channel.
- the process of FIG. 1B includes waiting for the primer liquid to flow through the microfluidic channel structure by capillary action.
- FIG. 1C schematically illustrates a primer drying phase during which the solvent evaporates to leave behind what becomes the primer layer.
- the composition of the primer layer may be selected to allow sufficient drying to be carried out within a reasonable time at room temperature, thereby avoiding the need for heating.
- the substrate may be held at an elevated temperature to enable or at least accelerate drying. Complete hardening of the primer may not be needed at this stage of the process, and may be deferred until the end of the electrode formation process.
- FIGS. 1B and 1C represent an example of the application of a primer layer to the microfluidic channel structure.
- FIG. 1D schematically illustrates the component after completion of the primer drying phase.
- a primer layer 16 has been formed to cover substantially the entire inner surface of the channel.
- the primer layer is thicker at the base of the channel than in the side walls, especially near the top of the side walls where the primer layer is significantly thinner, as schematically illustrated.
- the uppermost side wall regions of the channel may not be covered with the primer layer.
- FIG. 1E shows the channel 20 during a conductive liquid distribution phase.
- the channel 20, already coated with the primer layer 16, is at least partly filled with a solution 23 which is a liquid comprising a solvent-containing carrier medium in which electrically conductive particles are dispersed.
- a solution 23 which is a liquid comprising a solvent-containing carrier medium in which electrically conductive particles are dispersed.
- the conductive liquid 23 can be applied by micro-dispensing into the channel, e.g. with a syringe, micropipette or ink jet print head nozzle.
- the composition of the conductive liquid allows it to spread through the primer-coated channel by capillary action, resulting in a smooth and even coverage of the channel.
- the process step shown in and described with reference to FIG. 1E provides an example of introducing a conductive liquid to the primed microfluidic channel structure, the conductive liquid comprising a carrier medium including a solvent in which electrically conductive particles are dispersed. It also represents an example of waiting for the conductive liquid to flow through the microfluidic channel structure by capillary action.
- FIG. 1F schematically illustrates a conductive liquid drying phase during which the solvent of the conductive liquid, and any residual solvent in the primer layer, evaporates to leave behind what becomes the electrode layer 21.
- the composition of the conductive liquid may be selected to allow the drying to be carried out within a reasonable time at room temperature, thereby avoiding the need for heating.
- the drying step can alternatively be carried out by a number of methods known to those skilled in the art. Examples include drying in a convection oven or a hot plate, or lamp annealing (for example via an infrared lamp, a xenon lamp, or a laser such as a YAG, argon, carbon dioxide or excimer laser).
- the substrate may be held at an elevated temperature to enable or at least accelerate drying.
- the process step of FIG. 1F provides an example of evaporating the solvent from the carrier medium to allow the electrically conductive particles to form the electrode structure.
- a sintering phase may follow the conductive liquid drying phase in which the conductive particles present in the ink are fused together. The sintering also removes any remaining solvent in the primer and the conductive liquid.
- a separate sintering phase could be carried out for the primer layer prior to introduction of the conductive liquid 23, i.e. directly after the primer drying phase.
- the electrode layer 21 can be used as an electrode layer in an active or passive microfluidic device, but may also form any other feature, for example may form part of an antenna structure.
- the shape of the channel need not be approximately semi-circular in cross-section as illustrated. Other shapes may be used.
- the base and/or side walls of the channels may be flat or have flat portions.
- the channels may be formed with a V-groove.
- the technology is relevant not only for forming conductive features to control or sense flow in channels of microfluidic devices, but also for forming conductive features in other parts of microfluidic devices, such as reaction chambers or reagent reservoirs.
- Electrode layer can be formed recessed, as illustrated, or flush with the upper surface 12 of the substrate. This means that if further layers are bonded or otherwise formed on the upper surface of the substrate, the further layer does not need to be specially shaped with recesses or distorted to accommodate the electrode layer.
- the temperature of the evaporation step depends on the boiling point of the solvent. Suitable temperatures range from 50° C. to 200° C.
- the method of the present technology further comprises, following the evaporation step, the step of laminating the substrate with a cap layer to encapsulate or cover at least a part of the electrode structure.
- cap layer is not particularly critical to the present technology provided it is capable of adhering to the treated substrate.
- examples include organic polymers such as those described and exemplified above in relation to the substrate, and inorganic polymers such as PDMS.
- the cap layer is formed from the same material as that used to form the substrate.
- the cap layer can be bonded to the substrate by a number of techniques known to those skilled in the art. Suitable techniques include solvent bonding, gluing, laser welding and thermal welding. In one embodiment, lamination of the cap layer to the substrate (for example, to cover at least a part of the electrode structure) is carried out using solvent bonding lamination. This method is particularly suitable when the substrate and cap layer are formed from the same organic polymer, especially cycloolefin copolymer.
- the process of solvent bonding is known to those skilled in the art and is essentially a two-step process as follows:
- the solvent is not particularly restricted provided it does not completely dissolve the substrate or cap layer.
- examples include aliphatic hydrocarbons such as hexane, heptane, octane, alicylic hydrocarbons such as cyclohexane, cycloheptane and decalin, aromatic hydrocarbons such as benzene, toluene and xylene, alcohols such as methanol, ethanol, 1-propanol, 2-propanol and 1-butanol, and mixtures thereof.
- a particular example is a 80:20 by volume mixture of ethanol and decalin, especially for those embodiments where the substrate and/or the cap layer are cycloolefin copolymer.
- the temperature of the press is not particularly restricted provided it is sufficient to enable the layers to join and does not cause the layers to completely melt or decompose. In one embodiment, the temperature is in the range from 40° C. to 200° C., in some embodiments 50° C. to 150° C.
- the pressure of the press is not particularly restricted provided it is sufficient to enable the layers to join and does not cause the layers to decompose.
- the pressure is in the range from 0.2 to 10 MPa, in some embodiments 0.5 to 5 MPa.
- the method of the present technology further comprises, after the lamination step, the step of applying radiation through the cap layer to cure the radiation curable monomer and thus harden the conductive liquid.
- the radiation may be any suitable electromagnetic radiation, but is, for example, ultraviolet or visible light.
- the substrate and/or the cap layer may be transparent to the radiation used to cure the radiation curable monomer or prepolymer.
- the coalescing function is important, since it is typically the basis under which the main activity of the device is performed. It is typical to coalesce droplets from different streams, e.g. sample and reagent, to form a coalesced droplet in which a chemical or biological reaction takes place.
- Such a combined droplet is sometimes referred to in the art as a nanoreactor, not just when in the nanometre scale, but even when in the micrometre scale.
- Actuating or sensing electrodes may be arranged in, or to extend into, the flow channels to contact the fluid, or may be arranged outside the flow channels, adjacent thereto, so there is an insulating medium, e.g. the substrate material and/or air, between the electrode(s) and the droplet-containing carrier liquid.
- an insulating medium e.g. the substrate material and/or air
- actuating electrodes is used to refer to electrodes of an active component, whereas the term sensing electrode is used to refer to electrodes in a passive component.
- the magnitude of the electric field created in the flow channel is typically of the order of 106-108 V/m.
- Passive components may be fabricated from conductive patterning in which electric or magnetic fields are induced by the passage of droplets (inductive loop detector).
- inductive loop detector The usual range of components known from radio frequency (RF) device fabrication may be used, including inductive, resistive and capacitive elements, and combinations thereof.
- RF radio frequency
- a simple passive component would be an electrode pair either side of a channel connected to form a sensing circuit including the channel, wherein the resistance would be affected, typically decreased, when a droplet passes the electrode pair.
- Electrically conductive patterning may be used to fabricate electromagnetic sensors to integrate with the microfluidic device, such as a Hall sensor, which for example might be useful if the droplets were associated with magnetic beads.
- a Hall sensor which for example might be useful if the droplets were associated with magnetic beads.
- Another sensor type which can be used for sensing the passage of droplets is an antenna structure such as a bowtie antenna.
- An electrode may extend substantially at right angles to the flow channel and terminate a small distance away from the flow channel edge, or at the flow channel edge, or in the flow channel, or may extend right through the flow channel.
- a pair of electrodes can be provided both extending substantially at right angles to each other and terminating opposed to each other on either side of the flow channel.
- Electrodes may extend in the flow channel direction and either be located in the flow channel or adjacent the flow channel.
- a pair of electrodes may be arranged to extend parallel to a channel on either side of the channel for a section of the channel so that an electric field may be applied transverse to the flow direction over the section of the flow channel.
- a wide range of droplet diameter is also envisages including the nanometre range, in particular 100-1000 nanometres, as well as 1-1000 micrometres, in particular 1-100 micrometres.
- the carrier liquid may be an oil.
- the droplet liquid may be an aqueous solution, e.g. containing an enzyme, or an alcohol solution, or an oil solution.
- FIG. 2A is a plan view of a part of a microfluidic device incorporating a pair of electrodes manufactured as shown in FIG. 1F .
- a portion of a microfluidic flow channel 30 is shown in which the flow direction may be considered left to right in the drawing.
- the flow channel 30 is filled in use with a carrier liquid 26 in which is immiscibly suspended a series of droplets 24 of active liquid, e.g. of an analyte.
- a first electrode channel 20A is arranged on one side of the flow channel and extends transverse to the flow channel and terminates a distance ⁇ from the adjacent rim or edge of the flow channel 30.
- a second electrode channel 20B is arranged on the other side of the flow channel co-linear with the first electrode channel 20A and also terminates a distance ⁇ from its adjacent rim or edge of the flow channel 30.
- the first and second electrode channels 20A, 20B arranged either side of the flow channel have conductive liquid layers therein (not separately illustrated) which are formed in the manner described further above, and thereby form a pair of electrodes which can be externally actuated or sensed in order to control or sense the flow of the liquid droplets in the flow channel.
- FIG. 2B is a section through the chain-dotted line AA of FIG. 2A from which the structure of the flow and electrode channels is evident.
- FIG. 2C is a section through dotted line BB of FIG. 2A which is identical to FIG. 1F , i.e. shows the structure of the electrode channel with primer layer 16 and electrode layer 21.
- FIG. 3 is a plan view of a part of a microfluidic device incorporating a pair of electrodes having an alternative topography to that of FIG. 2A .
- the electrode channels 20 ⁇ , 20 ⁇ have a different shape than in the example of FIG. 2A . Namely, each electrode is formed in a continuous channel portion of V-shape with the base of the V being arranged adjacent the flow channel 30.
- FIG. 4 is a plan view of a part of a microfluidic device incorporating a pair of electrodes having another alternative topography.
- the electrodes on either side of the flow channel 20 ⁇ , 20 ⁇ are each formed from a continuous channel portion in a digital, i.e. flat-based, U-shape, so the part of the electrode that is adjacent the flow channel is defined by a portion of the electrode channel that extends parallel to the flow channel.
- continuous channel portion shapes may also be employed. Having the part of the electrode that is adjacent the flow channel formed by a continuous channel portion has the advantage during fabrication that more even capillary flow of the conductive liquid will take place.
- FIG. 5 is a schematic plan view of a component of a microfluidic device for generating droplets on demand.
- a fluid reservoir 32 holds a volume of the active liquid (shaded) from which droplets 24 are formed.
- a pair of electrodes 20A, 20B are placed adjacent to a constricted channel portion 34 arranged between an outlet of the reservoir 32 and a flow channel 30. Absent actuation of the electrodes 20A, 20B the active liquid is in equilibrium with a meniscus 35 being formed in the constricted channel portion 34.
- Droplets may be produced on demand in this way, for example a series of droplets may be produced by repeatedly applying voltage pulses to the electrodes.
- FIG. 6 is a schematic plan view of a component of a microfluidic device for coalescing pairs of droplets received from first and second channels.
- First and second inlet flow channels 30A and 30B combine as viewed in the direction of flow at a Y-junction 37 to form a single combined flow channel 30C.
- a series of droplets 24 of a first active liquid are received from the first inlet flow channel 30A.
- a series of droplets 25 of a second active liquid are received from the second inlet flow channel 30B.
- the droplets 24, 25 are carried by a carrier liquid 26.
- the two series of droplets are controlled so that they arrive in adjacent pairs in the flow channel 30C, i.e. with slightly offset arrival times, as illustrated.
- An electrode pair 20A, 20B is arranged at a point in the flow of the flow channel 30C.
- the electrodes are selectively actuated with a voltage pulse at times when droplet pairs 24, 25 pass by so as to cause each droplet pair to coalesce into a combined droplet 27 (cross-hatched).
- the mixture of the first and second liquids may serve to activate or deactivate a chemical reaction or a biological process depending on the application.
- FIG. 7 is a schematic plan view of a component of a microfluidic device for routing or sorting droplets at a channel T-junction 39.
- a series of droplets 24 of an active liquid (shaded) carried in a carrier liquid 26 arrive along a flow channel 30A at the T-junction 39 at which the flow splits into a left flow channel 30B and a right flow channel 30C.
- a left electrode pair 20A, 20B is arranged part way along the left flow channel 30B and a right electrode pair 20C, 20D is arranged part way along the right flow channel 30C.
- the left and right electrode pairs are operated in tandem to apply an electric field either in the direction shown with the arrow 31 or the opposite direction in order to route the droplets 24 arriving along channel 30A down the left channel 30B or the right channel 30C (as illustrated).
- a sensor 38 can be arranged in the flow upstream of the T-junction, as schematically illustrated, to measure a property of each droplet on the basis of which sorting is to be performed. Individual droplets may then be directed down the left or right flow channels 30B, 30C depending on their measured properties.
- the sensor 38 could be an electromagnetic sensor formed with conductive liquid elements made according to the method described herein, or could be an unrelated type of sensor, such as a sensor operable to make an image-based measurement (i.e. camera or microscope with image processing) or a spectroscopic measurement.
- FIG. 14 may be understood that further embodiments may combine the previously discussed embodiments and include conductive liquid patterning on both sides of the substrate.
- some components such as antennas or surface RF components such as RLC components, may be beneficially fabricated on a planar surface, i.e. typically the substrate's lower surface 14, whereas electrodes that extend into the flow channels to form conductive paths including liquid in the flow channels will need to be fabricated on the substrate's upper surface 12 where the flow channels exist.
- the above-described method of forming patterned conductive layers can be used outside the field of microfluidic devices to form electrode structures or other electrically conductive patterns when fabricating other kinds of device, in particular when polymer substrates are used.
- FIGS. 8A to 8F are schematic views of steps in a method for fabricating a credit card format contactless smart card with embedded antenna.
- FIG. 8A is a schematic plan view of a substrate 10 for a credit card format contactless smart card with a channel 20 formed to create an antenna.
- the substrate 10 has an upper or top surface and a lower or bottom surface.
- the channel 20 is in a shape to form an antenna structure with a double coil or winding adjacent the lateral periphery of the smart card.
- An additional depression or pad 40 is formed which is to provide a second contact to a chip that will be embedded in the finished smart card.
- the first contact will formed by the adjacent end of the channel at location (pad) 41.
- the area to be occupied by the chip is shown with the dotted rectangle.
- FIG. 8B shows the substrate after the channel 20 has been filled by capillary action first with a primer liquid and then with a conductive liquid in the same way as described above in connection with FIGS. 1A-1G .
- the two solutions can be applied by micro-dispensing into the channel 20 to form the first contact 42 and antenna structure 44 and separately to the depression 40 to form the second contact 46.
- the dispensing can be with a syringe, micropipette or ink jet print head nozzle.
- the composition of each solution allows it to be applied to the channel by capillary action, resulting in a smooth and even coverage of the channel and depression. After drying and sintering the conductive particles are fused together and form an effective electrically conducting path.
- FIG. 8C schematically illustrates the next step in the process in which an insulating film 48 has been deposited, for example by vapour deposition or printing, on a local region of the antenna structure 44.
- primer is printed, evaporated or otherwise deposited on top of the insulating film, the primer having similar properties to the primer liquid dispensed by capillary action in the previous step.
- FIG. 8D schematically illustrates the next step in the process in which a conductive strip 50 is deposited, for example by vapour deposition or printing, on the insulating film 48 to connect the second contact pad 46 with the antenna so that a complete two turns of conductor are formed between the first and second contacts 42 and 46.
- FIG. 8E schematically illustrates an intermediate layer 50 with an aperture 52 for receiving the chip.
- FIG. 8F shows a final assembly step in which the chip 54 is mounted on its contacts 42 and 46, the intermediate layer 50 is bonded to the upper surface 12 of the substrate 10, and a cap or laminating layer 56 is bonded to the intermediate layer 50 and substrate 10.
- the lower surface of the substrate 10 is also indicated with reference numeral 14.
- the antenna electrode is formed substantially flush with the upper surface 12 of the substrate, so that the intermediate layer 50 can be bonded directly onto the upper surface of the substrate 10 without needing recesses to accommodate the antenna electrodes 44 and contact pads 42 and 46 and without needing solvent-based softening to induce accommodating distortion.
- the contactless smart card may for example comply with ISO 14443 or ISO 15693 for example.
- the chip may be an RFID (radio frequency integrated circuit) chip for example operating at a frequency of 50 MHz or 14.5 MHz.
- two adjacent antennas may be provided on the smart card with appropriate individual frequencies to resonate at a resonant frequency of, for example, 13.56 MHz.
- a second antenna could be formed on the underside of the laminating layer 56 using the same process as is used to form the antenna on the substrate 10.
- FIG. 9 is a schematic plan view of a substrate for forming a pair of interdigitated channels 60 and 62 to form electrodes of the same shape.
- the channels 60 and 62 have respective contact pad areas 61 and 63 which as well as forming suitable areas for connection to other circuit elements in a finished device, such as an electrical supply or to a sensor, provide suitable areas for deposit of primer and then conductive liquid in droplets.
- the respective liquid can then disperse throughout the respective channels by capillary action to form a pair of interdigitated electrodes having the pattern shown with the electrodes interdigitating over a distance d.
- Interdigitated electrodes are common features in different applications, including for microfluidic channels, for addressing one- and two-dimensional touch sensors, and address lines for LED and LCD displays.
- channels or depressions of suitable shape can be provided for forming arbitrary shaped conductive features, including: polynomial or cloverleaf electrodes; castellated electrodes; spirals of various forms including circular, square, hexagonal and octagonal as are used to fabricate inductors in RF circuits; patterns for fabricating capacitors in RF circuits such as lateral flux capacitors formed of interdigitating electrodes and fractal capacitors based on Minkowski sausage; and the rich variety of patterns used for electrodes in touch sensors.
- the pad width ranges from 10 ⁇ m to 1 mm, in some embodiments 100 ⁇ m to 500 ⁇ m.
- the channel width ranges from 1 ⁇ m to 100 ⁇ m, in some embodiments 2 ⁇ m to 50 ⁇ m.
- the channel spacing ranges from 1 ⁇ m to 100 ⁇ m, in some embodiments 2 ⁇ m to 50 ⁇ m.
- the channel depth ranges from 1 ⁇ m to 100 ⁇ m, in some embodiments 2 ⁇ m to 50 ⁇ m.
- Electrode patterns were injection moulded in cycloolefin polymer according to the structure and dimensions shown in Test Pattern 1, shown in FIG. 10 .
- the schematic shows two types of electrode structures, each with four dispensing pads 1.60 mm in diameter.
- the electrode patterns vary in channel depth and width, according to Table 1. These electrode patterns were used for primer dispensing and conductive liquid tests by capillary flow in the Examples which follow.
- conductive liquid jet inks were dispensed only into the pads and the fluidic flow judged using a relative scale.
- the conductive liquid jet inks used contain silver nanoparticles, namely SunTronic EMD5603, available from SunJet Bath UK and Cabot CCI-300, available from Cabot Corporation USA.
- the flow of the conductive liquids in the preformed channels was judged for three criteria: (a) capillary flow of the fluid into the channel portion of the electrode pattern; (b) overflow of the fluid from the dispensing pad into the area surrounding the pad (an undesirable feature) and (c) formation of a complete electrode pattern by capillary action (all areas of the pattern filled uniformly with conductive liquid) as shown in FIG. 11 .
- the results are shown in Table 2 below.
- Comparative Example 1 The same test pattern as in Comparative Example 1 was used to gauge the effect of primer treated substrate on conductive liquid flow, a direct comparison with Comparative Example 1-a test with and without primer.
- Three primers were made according to the present technology using the following procedure and tabulated formulations.
- Copolymer 958 (a copolymer of vinyl pyrrolidone and dimethylamino-ethylmethacrylate available from ISP), supplied as 50% by weight in ethanol, was diluted to 5% concentration by stirring in additional deionised water.
- Dispal 14N4-80 an alumina available from Sasol GmbH, is supplied in powder form. A dispersion of Dispal 14N4-80 at 5% concentration by weight in water was made with a high speed stirrer, adjusting the pH to 3-5 with glacial acetic acid to ensure a uniform dispersion.
- the two preparations now both at 5% concentration by weight, were blended together using a high speed stirrer in three ratios as defined in Table 3 (listed in the second and third column are the parts by weight of the Copolymer 958 solution to the parts by weight of the Dispal 14N4-80 dispersion).
- the resulting preparations are denoted in Table 3 as "Primer Conc A, B and C”.
- Each primer concentrate was further diluted in a ratio of 1 part by weight concentrate to 4 parts by weight isopropoxyethanol as shown in column 4.
- the solvent addition provides the desired viscosity and surface tension for ideal fluidic flow of the primer in the electrode structures, so as to achieve uniform coverage of the primer in all areas of the test patterns.
- the primer was dispensed only in the pad areas of the patterns shown in FIG. 10 , and allowed to flow via capillary action into all regions of the pattern.
- Primer A is more effective for promoting conductive liquidic flow in the wider channels, whereas Primer B is more effective in the narrower channels.
- Primer C has broad effectiveness but its function is more sensitive to channel geometry specifics. It is clear that matching primer and channel geometry influences conductive liquidic flow, and in the majority of cases the primer has improved the fluidic flow compared to the control (the results of Comparative Example 1, shown in Table 2).
- Example 2 To further substantiate Example 1, further tests were carried out to establish the relationship between polymer concentrations in the primer and conductive liquid flow.
- the primer formulations designated in FIG. 12 as "polymer Concentration 5-20 inclusive can be found in Table 5.
- test conditions were an exact repeat of those in Example 1, only the measurement criteria was changed to "ink flow rate", i.e. extent of coverage with time.
- the silver nanoparticle ink jet ink, SunTronic EMD5603 was once again used as a conductive liquid and dispensed on the dried primer, again on the test pattern of FIG. 10 .
- Primer B yields the overall best result for effective channel filling with a commercial conductive liquid in the channel geometry range of 18-42 ⁇ m width and 70-150 ⁇ m depth in cycloolefin polymer.
- the test pattern in FIG. 13 was injection moulded in polymethyl methacrylate.
- the fluidic flow of Suntronic EMD5603 was characterised in terms of whether the channel portions of the test design could be completely filled by capillary flow by dispensing the fluid only the pad area of the test design without primer treatment, If the channel could be completely filled, the time taken to do so was recorded.
- Dispal 14N4-80 at 10% concentration by weight in water was made on a high speed stirrer, adjusting the pH to 3-5 with glacial acetic acid before adding the powder to the water to ensure a uniform dispersion.
- the Dispal 25SR is an organically modified alumina and therefore better suited for solvent based dispersions.
- the technique for creating a dispersion using a high speed stirrer was also used for this material, but the 10% concentrate was made in isopropoxyethanol.
- primers F and G the dilution ratio was the same, but the primers were diluted with a 50:50 blend of isopropoxyethanol and dipropylene glycol monomethyl ether, thus enabling a direct comparison of the diluents' composition.
- the primers listed in Table 8 were dispensed into the pad area of the injection moulded test pattern defined in FIG. 13 and the flow rate along the connecting channel measured. The flow rate was found to be in the following order: Primer G>Primer F>Primer E>Primer D.
- a non-treated pattern was dispensed with conductive liquid so as to judge the effect of the primer treated channels.
- the test criteria is demonstrated in FIG. 15 using primers D and E as examples, the figure illustrates how extent and rate of fluidic flow can be simply compared.
- flow rate is directly proportional to surface coverage-fast flow rate also implies effective coverage ("wetting") and dried primer composition.
- the organically modified alumina yielded the most effective primer for the conductive liquid containing a radiation curable component.
- the test pattern shown in FIGS. 16 a and 16 b was injection moulded in cycloolefin polymer.
- the dimensions of the test pattern are set out in Table 10.
- TABLE 10 A B C D 1 w: 10 p: 200 w: 10 p: 200 w: 5 p: 200 w: 10 p: 250 d: 5 t: 10 d: 5 t: 20 d: 5 t: 10 d: 5 t: 20 2 w: 10 p: 200 w: 10 w: 200 w: 200 w: 5 p: 200 w: 10 p: 250 d: 10 t: 10 d: 10 t: 20 d: 10 t: 10 d: 10 t: 20 3 w: 10 p: 200 w: 10 p: 200 w: 5 p: 200 w: 10 p: 250 d: 20 t: 10 d: 20 t: 20 d: 20 t: 10 d: 20 t: 20 4
- FIG. 16 a depicts a test electrode pattern used to evaluate microfluidic flow on a smaller scale than in Examples 1-3 and Comparative Examples 1 and 2.
- the pattern has essentially eight dispensing pads connected by four channels-hence two dispensing pads per channel, one on the left of the channel and one on the right.
- FIG. 16b also depicts the pad area of the same electrode pattern, this area was used for dispensing and the extent of fluidic flow in the microfluidic channels was judged in the same way as explained in the previous comparative examples.
- Table 10 defines the dimensions of each electrode pattern tested-labelled A1 through to D6, therefore 24 test patterns in total.
- FIGS. 17 a to 17 c illustrate the results of depositing conductive liquid by ink jet printing into pads without primer.
- primer G and the conductive liquid according to Table 9 is a simple and effective combination for filling channel widths of at least 5 ⁇ m width and possible less. No overflow into neighbouring channels was observed.
- the channel geometry has an influence on successful microfluidic flow when the dimensions are in the sub 10 ⁇ m range; the summary table indicates the channel depth must at least be equal to the width.
- the present technology may also be carried out using gold as the metal in the conductive liquid.
- FIG. 19 shows gold filling according to the present technology.
- Metals absorb electromagnetic radiation and dispersions of metallic nanoparticles absorb selective wavelengths of radiation depending on their particle size. There is strong UV absorbance for silver nanoparticles with particle sizes of ⁇ 80 nm, with a strong decrease for the same particle size distribution at around 500-550 nm. As the wavelength increases, the absorbance decreases regardless of particle size. Therefore, for metal nanoparticles (particularly silver nanoparticles) in a functional conductive liquid a curing mechanism "window" exists in the visible green to red region of the electromagnetic spectrum.
- a visible light curing system may be used based on light absorbing dyes-radical producing photoinitiators that facilitate free radical polymerisation.
- the dye absorbs the light energy, the excited dye then undergoes energy and/or charge transfer reactions with a coinitiator.
- the coinitiator in turn produces the reactive radical species that initiates photopolymerisation of reactive monomers and/or prepolymers.
- the polymers based on vinyl lactam and PVAc/VC were dissolved in solvent. Ethanol was used to dissolve the lactams and a mixture of methyl ethyl ketone and toluene was used to dissolve the PVAc/VC.
- the dye and coinitiator were dissolved in ethanol: the maximum solubility of Basic Red 2 in ethanol is 3% by weight and the aminobenzoate was used as a 12% solution.
- the two premixes were added together to form a dyed polymer coating wherein the dye concentration is 1% based on the solid polymer.
- the coatings were applied by Mayer bar to polycarbonate to form a 10 ⁇ m dry film. UV/Visible spectra were taken using a Perkin Elmer Lambda 9 and the photosensitivity of the coatings was established using Hoya Ex 250 UV light source.
- the dye may be evenly distributed throughout the polymer and in close contact with the coinitiator.
- the spectra shown in FIGS. 21 and 22 show how dye decomposition can be controlled by the polymer support and by the amine coinitiator.
- the spectrum of the dye in the polymer support based on vinyl pyrrolidone copolymer has no evidence of aggregation and the dye is rapidly decomposed by irradiation.
- a vinyl lactam polymer may be used.
- the vinyl lactams lead to more effective curing because aggregation of the visible light absorbing dye is avoided and unwanted photophysical effects can be reduced.
Claims (9)
- Procédé de fabrication d'un dispositif ayant une structure d'électrode, le procédé comprenant :a) fournir un substrat (10) ayant une structure de canal microfluidique (20) formée pour correspondre à la structure d'électrode;b) appliquer à la structure de canal microfluidique une couche d'apprêt (16) qui comprend un matériau particulaire poreux et ne comprend pas de polymère organique, la couche d'apprêt étant capable d'absorber un solvant organique humectant dans lequel des particules métalliques d'un liquide conducteur (23) sont dispersées;c) l'introduction du liquide conducteur (23) sur la structure de canal microfluidique apprêtée, le liquide conducteur comprenant des particules électriquement conductrices dispersées dans un milieu porteur comprenant un solvant organique humectant qui est absorbable par la couche d'apprêt;d) attendre que le liquide conducteur s'écoule dans à travers la structure de canal microfluidique par action capillaire; ete) évaporer le solvant organique humectant du milieu porteur pour permettre aux particules électriquement conductrices de former la structure d'électrode (21); etf) fritter le substrat (10) ayant la structure de canal microfluidique (20) pour fusionner les particules conductrices et pour enlever tout solvant organique humectant restant; etg) stratifier le substrat avec une couche de recouvrement pour recouvrir au moins une partie de la structure d'électrode.
- Procédé selon la revendication 1, dans lequel le solvant est un solvant organique miscible avec l'eau.
- Procédé selon la revendication 2, dans lequel le milieu porteur contient en outre de l'eau.
- Procédé selon la revendication 2, dans lequel le solvant organique est un solvant oxygéné choisi parmi un alcool, un éther de glycol et un ester de glycol.
- Procédé selon la revendication 1, dans lequel dans l'étape (a) un tampon est en outre formé sur le substrat en communication fluidique avec le canal microfluidique, et dans l'étape (c) le liquide conducteur est appliqué sur le tampon et distribué à la structure de canal microfluidique par action capillaire.
- Procédé selon la revendication 1, dans lequel le substrat est un polymère organique.
- Procédé selon la revendication 1, dans lequel dans l'étape (a) le substrat ayant un canal microfluidique est formé par moulage par injection.
- Procédé selon la revendication 1, dans lequel l'étape (b) d'appliquer la couche d'apprêt comprend :b1) introduire un liquide d'apprêt dans la structure de canal microfluidique, le liquide d'apprêt comprenant un milieu porteur d'apprêt comprenant un solvant d'apprêt; etb2) attendre que le liquide d'apprêt s'écoule à travers la structure de canal microfluidique.
- Procédé selon la revendication 8, dans lequel :l'étape b2 comprend (b2) attendre que le liquide d'apprêt s'écoule à travers la structure de canal microfluidique par action capillaire; etl'étape (d) comprend attendre que le liquide conducteur s'écoule à travers la structure de canal microfluidique par action capillaire.
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DE102014107480B4 (de) * | 2014-05-27 | 2016-02-04 | Webasto SE | Kunststoffheckscheibe mit Heckscheibenheizung und Verfahren zur Herstellung derselben |
CN106471073B (zh) * | 2014-07-03 | 2021-11-23 | 康宁股份有限公司 | 喷墨组合物、方法以及经过涂覆的制品 |
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US20180221873A1 (en) * | 2015-12-14 | 2018-08-09 | Hewlett-Packard Development Company, L.P. | Microfluid channel with developer port |
JP6654951B2 (ja) | 2016-03-31 | 2020-02-26 | 株式会社エンプラス | 流体取扱装置 |
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WO2020160343A1 (fr) * | 2019-01-31 | 2020-08-06 | Samtec, Inc. | Trous métallisés électroconducteurs et leurs procédés de production |
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US9823221B2 (en) | 2017-11-21 |
US20150014170A1 (en) | 2015-01-15 |
EP2814610A1 (fr) | 2014-12-24 |
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